JP6542247B2 - A single paste-type dental hydraulic filler composition - Google Patents

Description

  [1] The present invention relates to a single paste type dental hydraulic filler composition. More specifically, it relates to a single paste-type dental hydraulic filler composition comprising a hydraulic cement and a non-aqueous liquid, which absorbs moisture from the surrounding liquid and air and cures rapidly. It is a thing.

[2] Endodontics (endodontics) is a specific area of dentistry for the pathological treatment of dental pulp and apical tissue.
[3] Teeth include nerve and blood vessel tissue called dental pulp inside, dentin covering the dental pulp and the outermost hard enamel. Root canal treatment is given mainly when the dental pulp is infected.

  [4] Root canal treatment of teeth with inflammation in progress and teeth with pulp tissue that has undergone necrosis (access cavity, access), which is generally formed in a crown. The internal space of the tooth called the pulp chamber (pulp chamber) is opened via the cavity, and the root canal treatment instrument is introduced into the root canal inside the root.

  [5] After root canal treatment, seal the root canal with root canal filling to prevent secondary infection. An ideal dental root canal filling material is biocompatible (biocompatibility), bactericidal property, sealing property, stability (stability), workability (workability), dispersability (dispersion property) It is desirable that the characteristics such as easily placed and distributed property, radiopacity, etc. be excellent.

  [6] Gutta percha and sealer can be mentioned as examples of such root canal filling materials. Root canal treatment using gutta-percha and sealer is seen as a conservative therapy. This is usually used in two ways. One is lateral pressure and the other is vertical pressure. Lateral pressurization puts the gutta percha cone inside the root canal and pressurizes it laterally with a mechanism called a spreader to fill the root canal, and the empty space between the filled gutta percha and the root canal is a sealer. It is a way to pack it. Vertical pressurization is a method in which a gutta-percha is inserted into a root canal and pressurized vertically with a tool called a plugger to fill the root canal.

  [7] However, according to such a conventional method, there is a risk that the root may be broken or the root may be damaged in the process of applying pressure to the gutta-percha. Not only that, because the tooth has a complex and diverse shape of the root canal system, a more reliable seal is necessary.

  [8] On the other hand, if the general root canal treatment process can not be carried out normally, or depending on the condition and condition of the tooth, the infected tissue is appropriate as a non-surgical (that is, non-operative) treatment. If it can not be removed, surgical root canal treatment will be performed to maintain the teeth. In such cases, the most common practice is to cut the tip of the tooth root (that is, perform Apicoectomy) and form a reverse root canal filling cavity in the tip. And filled with artificial material. According to this, the tissue and bacteria present in the infected root canal are not transmitted to the tissue around the root (that is, the tissue around the root end), so the inflammation around the root end is prevented and the tooth is maintained for a long time can do.

  [9] A plurality of substances have been used as materials for filling the root of these roots at the root canal, but various biological / physical evaluations have been performed on them. As materials that can be considered, gutta percha, polycarboxylate cement (Polycarboxylate cement), amalgam (Amalgam), super EBA (Super-EBA), Cavit (Cavit), zinc oxide (Zinc oxide), eugenol (Eugenol), glass ionomer cement (Glasss-ionomer cement), zinc phosphate cement, etc. are known. However, some of these have been reported to lose physical properties for use in surgical environments where biocompatibility is low and blood and other fluids are present.

  [10] On the contrary, MTA (Mineral Trioxide Aggregate) cement is known as a material with excellent ecological compatibility and sealability. It can be used universally for the closure of the posterior root canal filling and perforation, pulp capping, pulpotomy, apexification (artificial apical barrier placement), It is positioned as a typical dental material used for procedures such as revascularization and revascularization and apexogenesis procedure. Therefore, various efforts have been made to fill the root canal with MTA cement that is hardened by water and has excellent sealing performance in a wet environment, and as part of this, it is possible to make MTA cement in paste form and use it There is an active research on Related to this, the technique of Patent Document 1 can be cited as an example.

  However, although the root canal is generally presumed to be a moist environment, many dentists are used to drying the root canal in the course of root canal treatment, so all the roots are The tubes are not always wet. Conventional MTA cement products need to be mixed with liquid just before being injected into the root canal, are cumbersome to use and have relatively poor flow and operability, and are located deep within the root canal Have the disadvantage of taking a long time to

  [12] Therefore, the present inventors have proposed a single paste-type MTA cement that absorbs surrounding moisture even in the dried root canal and reliably cures in an appropriate time. is there.

Korean Published Patent No. 10-2010-0037979

[13] The object of the present invention is to solve all the problems described above.
[14] Another object of the present invention is to provide a single paste-type dental filler composition that can be housed in a syringe that does not require a separate mixing process.

  [15] The present invention is a single paste-type dental filler composition which is easy to cure rapidly and three-dimensionally seal a root canal or tooth perforated site, and which is excellent in biocompatibility. Another purpose is to provide.

  [16] The present invention is a single paste-type dental filler composition capable of absorbing moisture from interstitial fluid and air in and around wet cotton and root canal and surrounding parts and curing them easily. Another purpose is to provide.

  [17] Another object of the present invention is to provide a safe single paste type dental filler composition which does not require application of heat and pressure.

[18] The typical configuration of the present invention for achieving the above object is as follows.
[19] According to one aspect of the present invention, a single paste-type dental hydraulic property comprising a hydraulic cement, a non-aqueous liquid having non-aqueous liquid (non-aqueous liquid, non aquaous liquid), and a radiopaque substance A filler composition is provided.

  [20] Other configurations may be further provided based on the technical idea of the present invention.

[21] According to the present invention, there is provided a single paste-type dental filler composition that can be stored and provided in a syringe that does not require a separate mixing process.
[22] According to the present invention, a single paste-type dental filler composition excellent in biocompatibility which is easy to harden rapidly and three-dimensionally seal the root canal or tooth perforated site. The goods are provided.

  [23] According to the present invention, a single paste-type dental filler composition capable of absorbing moisture from interstitial fluid or air in wet cotton or in a root canal or its periphery and curing easily. The goods are provided.

  [24] According to the present invention, a safe single paste type dental filler composition is provided without the need for heat and pressure.

[25] FIG. 1 is a graph according to Test Example 4 of the present invention.

  [26] The following detailed description of the invention refers to the accompanying drawings which show, by way of illustration, specific embodiments in which the invention may be practiced. These examples are described in detail to enable those skilled in the art to practice the present invention. It should be understood that the various embodiments of the invention, although different from one another, need not be mutually exclusive. For example, the particular shapes, structures, and characteristics described herein may be modified and implemented from one embodiment to another without departing from the spirit and scope of the present invention. Also, it should be understood that the location or arrangement of the individual components within each example may be varied without departing from the spirit and scope of the present invention. Accordingly, the detailed description given below is not to be taken in a limiting sense, and the scope of the present invention should be taken as covering the scope of the claims and all equivalent scope of the claims. You must. Like reference symbols in the drawings indicate like or similar components across several aspects.

  [27] In the following, reference will be made to the accompanying drawings of some preferred embodiments of the present invention in order to enable those skilled in the art to which the present invention pertains to easily practice the present invention. I will explain in detail.

[28] Preferred embodiments of the present invention [29] 1) Hydraulic cement [30] The filler composition according to the present invention is hardened by absorbing moisture in or around the root canal, and has excellent biocompatibility And hygroscopic hydraulic cement having sealing property.

  [31] The hydraulic cement can contain calcium oxide or calcium hydroxide as an active ingredient, and can preferably contain portland cement or pozzolanic cement. In particular, it may be desirable to include portland cement that is not only similar in physical properties and chemical composition to MTA, but also has superior biocompatibility.

  [32] It may be preferable to maintain the average particle size (D50) of the hydraulic cement to 3 microns or less in terms of flowability (flowability) and reactivity. It may be desirable that these hydraulic cements be contained in an amount of about 15 to 55% by weight based on the total composition.

  [33] In addition, the composition according to the present invention improves the hygroscopicity of the paste to enable high-speed and reliable curing, while maintaining biocompatibility and improving the sealing property, water There may be further added calcium chloride having hygroscopic and deliquescent properties of hard cement. In this case, it may be desirable that calcium chloride be contained in an amount of about 1.5 to 5.5% by weight based on the total composition.

  [34] Further, the composition according to the present invention may use pozzolanic cement in which water is used as crystal water in the process of hydration as in the following chemical formula, including an active silica substance in portland cement (For the composition of these pozzolanic cements, reference may be made to Korean Patent Application Publication No. 1000402 of the applicant (the content of this publication is incorporated in its entirety into the specification of the present application)).

[35] CaO + H ₂ O-> Ca (OH) ₂
[36] Ca (OH) ₂ + SiO _2- > CaO, SiO ₂ , n (H ₂ O)
[37] When using these pozzolanic cements, the composition contemplated by the present invention is achieved without the addition of calcium chloride with the help of the water of crystallization produced by the above formula. Can.

[38] 2) Non-aqueous liquid [39] The composition according to the present invention can include a non-aqueous liquid having hygroscopicity to paste hydraulic cement.

  [40] It is desirable that these non-aqueous liquids contain substantially no water that reacts with hydraulic cement to cause a hydration reaction, or contain only a minimal amount of water that does not cause hardening. Sometimes. In these non-aqueous liquids, it may be desirable for water to be included as much as only up to about 3% by weight relative to the non-aqueous liquid. Biocompatibility, storage stability, hygroscopicity, surface activity, the property of being easily mixed with water, the property of being rapidly absorbed into the human body, etc. may be required for the characteristics of the non-aqueous liquid.

  [41] Non-aqueous liquids having the characteristics as described above are N-methyl-2-pyrrolidone (N-methyl-2-pyrrolidone, ie, "NMP"), polyoxyethylene sorbitan monolaurate , Dimethyl isosorbide, diethylene glycol dimethyl ether (dilyme) (or diethylene glycol monoethyl ether (Carbitol Cellosolve)) and butylene glycol (butylene glycol) It may include at least one selected from Ranaru group, preferably, can include NMP.

  [42] These non-aqueous liquids are desirably contained in an amount of about 15 to 35% by weight based on the total composition. If the content is less than 15% by weight, it becomes difficult to secure appropriate flowability (flowability), and if it exceeds 35% by weight, the flowability (flowability) becomes very large and hydration occurs. Reaction may be hampered.

[43] 3) Radiopaque substance [44] The composition according to the present invention is a radiopaque substance, for example, barium sulfate, zirconium oxide, bismuth oxide, for ease of measurement. It may include at least one substance selected from the group consisting of tantalum oxide and calcium tungstate, but preferably it is bismuth oxidized for high levels of radiopacity and biocompatibility. It is desirable to use iron oxide or zirconium oxide.

[45] The radiopaque substance is desirably contained in an amount of about 20 to 55% by weight based on the total composition.
[46] 4) Hygroscopic clayiness [47] To ensure that the curing process is performed even in the extremely dry root canal with the combination of hygroscopic cement and hygroscopic non-aqueous liquid alone as described above. May be a bit short, so it is hygroscopic to meet higher hygroscopicity and other requirements of root canal fillings, such as adequate flowability (flowability), maneuverability, ultrasonic transmission, etc. It is desirable that the clay be further included (although such hygroscopic clay may not be a component that should necessarily be included).

  [48] The hygroscopic clay can include at least one selected from the group consisting of bentonite, smectite and synthetic clay minerals, preferably bentonite. Can be included.

  [49] Bentonite is composed of a large number of natural clays, so that viscosity stability and formation of a structure can be realized even over a wide temperature range, thereby improving resistance to sag and peeling and acting as a retarder. Improve the open time of Portland cement. It is resistant to bacteria and enzymes, and can also be antibacterial.

[50] It may be desirable that these hygroscopic clayey materials be contained in an amount of about 1 to 10% by weight based on the total composition.
[51] 5) Hygroscopic Thickener [52] The composition according to the present invention is prepared from hydroxyethyl cellulose, hydroxypropyl methyl cellulose, carboxymethyl cellulose, polyvinyl alcohol and polyvinyl pyrrolidone in order to impart suitable viscosity to non-aqueous liquids. It may further comprise at least one hygroscopic thickener selected from the group consisting of

  [53] These thickeners prevent paste separation, retain moisture, increase operability, and increase the degree of cohesion. It can act as a surfactant to help the root canal filling material penetrate deeply and help maintain the softness of the paste surface. In addition, it is excellent in storage stability particularly in resistance to bacterial molds.

[54] It may be desirable that these thickeners be included in an amount of 0.1 to 1% by weight based on the total composition.
[55] Below, the production example of the present invention will be described more specifically.

[56] Production Examples 1 to 3
[57] A powder is prepared by mixing 100 parts by weight of Portland cement, 20 parts by weight of bentonite, 10 parts by weight of calcium chloride and 100 parts by weight of zirconium oxide, NMP added with 2% by weight of methylcellulose, 7% by weight of polyvinyl alcohol A single paste-type dental hydraulic filler composition was prepared by mixing each of the added NMP and 7% by weight of polyvinyl pyrrolidone into the added NMP.

  [58] Each paste was stored in a syringe and shielded from air, and when exposed outside the syringe at the time of use, it absorbed moisture in the atmosphere of all 50% humidity and hardened within 2 days. The

[59] This shows that the composition according to the present invention is reliably cured in a humid environment.
[60] Production Examples 4 to 6
[61] 200 parts by weight of Endocem ZR (a product of one-to-one mixing of zirconium oxide with pozzolanic cement) and 20 parts by weight of bentonite to prepare a powder, NMP to which 2% by weight of methylcellulose is added, 7 weight to polyvinyl alcohol A single paste type dental hydraulic filler composition was prepared by respectively mixing NMP added with 10% and NMP added with 7 wt% of polyvinylpyrrolidone.

  [62] Each paste was stored in a syringe and shielded from air, and when exposed outside the syringe at the time of use, it absorbed moisture in the atmosphere of all 50% humidity and hardened within 2 days. The

[63] This shows that the composition according to the present invention is reliably cured in a humid environment.
[64] Among the above production examples, the following example tests were carried out using the filler composition produced according to Production Example 2 in particular.

[65] Test Example 1: Solubility Test [66] The solubility of the filler composition according to the present invention was measured by the following method based on the test method of ISO 6876: 2012 (E) 5.6.

  [67] First, a mixture of 2 g of filler composition and 0.02 ml of water is packed in a mold of diameter (20 ± 1) mm and thickness (1.5 ± 0.1) mm (37 ± 1) The weight was measured after the specimen was removed from the mold after storage in an oven at 150 ° C. for more than 150% of the cure time. Two test pieces of one dish were placed, and distilled water (50 ± 1) was poured and stored in an oven at (37 ± 1) ° C. for 24 hours. Take out the dish, filter the distilled water with filter paper, put it in a pre-weighed beaker, also put about 5 ml of distilled water in the dish holding the test piece, filter it, and then make the beaker (110 ± 2) Placed in an oven at 0 C to evaporate distilled water and then measure the weight after cooling the beaker at room temperature. The difference between the weight of the beaker and the weight of the beaker from which the distilled water had evaporated was recorded and this weight was viewed as the amount of the dissolved specimen. The amount of such test pieces was converted to% to determine solubility. The results are shown in Table 1 below.

  [68] Table 1

[69] Test Example 2: Size Change Test [70] Change in Size of Filler Composition According to the Present Invention by the Following Method Based on the Test Method of ISO 6876: 2001 (E) 7.6 Was measured.

  [71] First, 0.02 ml of water was mixed with 2 g of the filler composition, and the mixture was packed in a mold having an inner diameter of 6 mm and a height of 12 mm, and then the upper and lower were covered with a film and a glass plate. Mold and samples were measured for cure time while being stored in an oven at (37 ± 1) ° C. during cure. Once the coupons were cured, the top / bottom of the coupons were polished and flattened with the mold and then the coupons were removed from the mold. Measure the length of the test piece and store it in distilled water at (37 ± 1) ° C for 30 days, and then measure the length of the test piece, the percentage change in the original length, and its average. The results are shown in Table 2 below.

  [72] Table 2

[73] Test Example 3: Coating degree test [74] The coating degree of the filler composition according to the present invention was measured by the following method based on the test method of ISO 6876: 2012 (E) 5.5. .

  [75] First, a total of three sets of two glass plates were prepared, and the thickness of the two glass plates was measured to an accuracy of 1 μm using an electronic caliber caliper. Three minutes after dividing 0.05 ml of composition and raising to the center of the glass plate, the glass plate is covered and a load of 150 N is applied. At this time, it was confirmed that the sample was completely filled with the glass plate. After the load was removed after 10 minutes, the thickness of the glass plate was measured, and then the difference in thickness of the measured glass plate was calculated to obtain the film thickness. The results are shown in Table 3 below.

  [76] Table 3

[77] Test Example 4: pH test [78] 1) Measurement of pH of paste itself: The weight of the composition was measured, and the composition was immersed in 10 times distilled water to measure pH.

  [79] 2) Measurement of pH immediately after curing: 0.02 g of distilled water is added to 2 g of the composition and mixed, and a mold of diameter (15 ± 0.1) mm and depth (1.0 ± 0.1) mm The solution was fully cured and then removed from the mold, and then the pH was measured as in 1).

[80] 3) Measurement of pH 1 day after curing: The sample solution of 2) was stored in a (37 ± 1) ° C. incubator, and then the pH of the sample solution was measured 1 day after curing.
[81] 4) pH measurement after 7 days of curing: store the sample solution of 2) in a (37 ± 1) ° C. after measurement of 3) is finished, and then measure the pH of the sample solution after 7 days of curing did.

[82] The averages of the pHs of the three sample solutions of 2) to 4) were determined, and the results are shown in the following Table 4 and FIG.
[83] Table 4

  [84] The present invention has been described above by means of specific items such as specific components and limited examples and drawings, which are provided to assist the more general understanding of the present invention. Only The present invention is not limited to the above-described embodiment, and various modifications and changes can be made from such description as long as the person skilled in the art has ordinary knowledge in the technical field to which the present invention belongs.

[85] Therefore, the spirit of the present invention should not be limited to the embodiments described above, and should be determined not only from the claims described below, but also from the claims or equivalent thereof. The entire scope of the modifications can be said to fall within the scope of the inventive concept.

Claims (12)

A dental hydraulic filling material, 20 to the whole composition to a hydraulic cement 15-55% by weight, the non-aqueous liquid having a hygroscopic 15-35% by weight, the radiological impermeable material A single paste-type dental hydraulic filler composition comprising 55% by weight and 1 to 10% by weight hygroscopic clay . The single-paste dental hydraulic filler composition according to claim 1, wherein an average particle size (D50) of the hydraulic cement is 3 μm or less. The single-paste dental hydraulic filler composition according to claim 1, wherein the hydraulic cement contains calcium oxide or calcium hydroxide as an active ingredient. The single-paste dental hydraulic filler composition according to claim 1, wherein the hydraulic cement comprises portland cement or pozzolanic cement. The non-aqueous liquid may be N-methyl-2-pyrrolidone (N-methyl-2-pyrrolidone, ie, "NMP"), polyoxyethylene sorbitan monolaurate, dimethyl isosorbide And at least one selected from the group consisting of diethylene glycol dimethyl ether (diglycol), diethylene glycol monoethyl ether (Carbitol Cellosolve) and butylene glycol A single paste-type dental hydraulic filler composition according to claim 1. The single radiopaque material according to claim 1, wherein the radiopaque material comprises at least one selected from the group consisting of barium sulfate, zirconium oxide, bismuth oxide, tantalum oxide, and calcium tungstate. Paste-type dental hydraulic filler composition. The single paste type according to claim 1 , wherein the hygroscopic clayey material comprises at least one selected from the group consisting of bentonite, smectite and synthetic clay minerals. Dental hydraulic filler composition. The single-paste dental hydraulic filler composition according to claim 1, wherein the non-aqueous liquid comprises a hygroscopic thickener. The single-paste hydraulic hydraulic filler composition according to claim 8 , wherein the numerical value of the percentage by weight of the hygroscopic thickener relative to the total composition is 0.1-1. 9. The single paste-type dental hydraulic property according to claim 8 , wherein the hygroscopic thickener comprises at least one selected from the group consisting of hydroxyethyl cellulose, hydroxypropyl methyl cellulose, carboxymethyl cellulose, polyvinyl alcohol and polyvinyl pyrrolidone. Filler composition. The single paste-type dental hydraulic filler composition according to claim 1, wherein calcium hydroxide having hygroscopicity and deliquescent properties of the hydraulic cement is added. The single-paste-type dental hydraulic filler composition according to claim 11 , wherein the value of weight percent relative to the total composition of calcium chloride is 1.5 to 5.5.